QuEChERS/超高效液相色谱-串联质谱法测定黑木耳中33种除草剂残留

Simultaneous Determination of 33 Herbicides Residues in Auricularia auricula by QuEChERS and Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry

[目的]建立一种基于QuEChERS(Quick Easy Cheap Effective Rugged and Safe)前处理技术和超高效液相色谱-串联质谱(UPLC-MS/MS)同时测定黑木耳中33种除草剂残留量的分析方法。[方法]黑木耳提取液采用分散固相萃取净化,UPLC-MS/MS测定,电喷雾电离,多反应监测模式检测。[结果]33种除草剂在1.0(2.0)~100(200)μg/L质量浓度范围内线性关系良好,相关系数均不小于0.9990;3个加标水平(0.020、0.040、0.200 mg/kg)的平均回收率为72.2%~122.7%,相对标准偏差(RSD)为0.8%~13.4%;检出限为0.003~0.015 mg/kg。[结论]该方法简单、快速、准确、灵敏度高,可用于大批黑木耳中除草剂残留快速检测。

[Aims] This study aims to establish a method for simultaneous determination of 33 herbicide residues in Auricularia auricular by QuEChERS(Quick Easy Cheap Effective Rugged and Safe) and ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS). [Methods] The extract of A. auricular sample was purified by QuEChERS method. UPLC-MS/MS method was performed with electrospray ionization(ESI) source under the multiple reaction monitoring(MRM) mode. [Results] The linear correlation coefficients were no less than the relative Standard devia tion(RSD) ranged from 0.8 to 13.4% at 0.9990 with the concentration range of 1.0(2.0)-100(200) μg/L.The average recoveries ranged from 72.2 to 122.7% and the relative standard deviation(RS) ranged from 0.8 to 13.4% at the addition levels of 0.020, 0.040 and 0.200 mg/kg. The limits of detection ranged from 0.003 to 0.015 mg/kg.[Conclusions] This method is easy operation, rapid, good sensitivity and accuracy, which is suitable for the simultaneous detection of herbicide residues in a large number of A. auricular samples.